Process for producing alkali metals or the like.



W. L. MORRISON.

PROCESS FOR PRODUCING ALKALI METALS OR THE LIKE.

APPLICATION FILED me. It, 1916.

l zy-Z I anucwroi MJA 6 Patented May 7, 1918.

3 SHEEYSSHEET I.

W. L. MORRISON.

CESS FOR PRODUCING ALKALI METALS APPLXCATHJN FILED AUG.1I.\9\6- F.

Patented May 1,1918.

PRO OR THE LIKE.

anuanfoz M anon/1MP W. L. MORRlSON. PROCESS FOR PRODUCING ALKALI METALS OR THE LIKE.

Patented May 7, 1918.

a SHEETSSHEET a Smucfll'o: w ll; W 351 flflowel p APPLICATION FILED AUGJI. 1916- UNITED STATE S PATENT OFFICE.

WALTER I. MORRISON, F CANONSBURG, PENNSYLVANIA, ABBIGNOB '10 ELECTRIC REDUCTION COMPANY, A CORPORATION OF DELAWARE.

PEDGEBS FOR PRODUCING ALKALI METALS OR THE LIKE.

Specification of Letters Patent.

Patented May 7, 1918.

Application filed August 17, 1816. Serial No. 115,882.

To all 'u'hom it may concern:

ducing Alkali Metals or the like, of which the following is a specification.

The invention relates to an improved process for producing metals, and more particularly for the production of alkali metals, such as sodium and potassium. The main object of the invention is to provide an improved process for the obtaining of such metals in a simple and etlicient manner, rapidly and without expensive apparatus. More specific objects, features and advantages will more clearly appear from the detailed'deseription given below, taken in connection with the accompanyilug drawings, which form a part of this specification.

In the drawings Figure 1 illustrates an apparatus, partly in section, in which the preliminary treatment of the material may be carried out. Fig. 2 illustrates an apparatus, partly in section, in which the material obtained from the apparatus of Fig. 1 is heated and the vapor of the metal produced and condensed. Fig. 3 is a framentary section of a part of the apparatus shown in Fig. 2. taken on the line XX of Fig. 2. Fig. 4 is a view, mostly in section, of an apparatus, by means of which the metal 0 tuined from the apparatus in Fig. 2 may be oxidized to peroxid. Fig. 5 is a section taken on the line Y-Y of Fig. 4.

While the improvements are adapted to the production of various metals 'and peroxids thereof, yet they are particularly applicable to the production of alkali metals, and in order that the invention and its a plication may be clearly understood, I Wlll describe them as applied to the production of metallic sodium and peroxid of sodium.

While any suitable compound of sodium may be used as a starting material, I prefer to use caustic soda or sodium hydrate, heeause of its cheapness and the ease with which it lends itself to the process. The sodium hydrate I mix with a suitable dehydrating agent. For this urpose I preferably use silicon in the iorm of ferrosilicon (90% silicon). Both of these mate rials are first preferably finely ground and then mixed in the molecular proportion of This mixed mass may be then caused to re act by touching the same with a red hot iron. The vigorous reaction which results progresses throughout the mass, liberating large quantities of hydrogen and rendering the mass red hot. The hydrogen may be collected and used for any desired purpose. The reaction which occurs is believed to be as follows:

Thus a basic sodium silicate is formed, together with some sodium oxid, which is more or less combined with the basic sodium silicate. The mass, on cooling, remains as a granular sandy residue, which is ground to a fine powder, and is then ready for the second step or treatment of the process.

This first treatment, as above explained, may be carried out in any suitable rece tacle, such as a large cast iron pan, but i? it is desired to have the process continuous, and collect the hydogen produced, an apparatus such as shown in Fig. 1 may be used.

Referring to Fig. 1, 1 represents a cast iron chamber provided with a water jacket 2, for kee ing the same cool. The chamber 1 is provided with a top 3, having a cover 4 which may be removed for the introduction of the material. The upper part of the chamber is provided with a water-jacketed partition 5, having an opening 6 adapted to be closed by a valve 7, operated by a lever 8. Below the partition 5 is another water-jacketed partition 9, having an 0 ioning therethrough adapted to be closed y a valve 10, operated by a lever 11. Below the partition 9 are water-jacketed protecting baflles 12.

Leading from the top of the apparatus is a pipe 13, which is connected to a vacuum pump. In the bottom of the apparatus there is arranged a cut-fli ht conveyer 14 of heavy construction, exten ing laterally through a cooling tunnel 15, having connected at its other end a ipe 16 provided with a gate valve 17. leading to an air-tight container 18, provided with an outlet 19 at its lower and, normally closed by a valve 20. A bygas tank 24, for the storage of the hydrogen gas produced by the process.

The caustic soda and ferro-sihcon being introduced through the opening covered by the cover 4. fall upon the partition 5. Upon replacing the cover 4, the air is exhausted from the space above the partition 5, then the valve 7 is operated to allow the material to fall upon the partition 9 and the air again exhausted. The valve 7 being closed, valve 10 is then opened and the ma.- terial falls upon the baffles 12, and from them drops to the bottom of the chamber 1.

The reaction may be initiated by heating this material by passing current through an electrical resistance wire extending into the bottom of the chamber 1, and after the reaction is thus once initiated, then, as further material is introduced into the chamber, as above explained, it falls upon the hot material at the bottom and the reaction is thus substantially continuous. The cut-flight conveyer 14, which is of low pitch, more or less cuts up the lumps of the material and at the same time feeds it to the pipe 16, so that it drops into thecontainer 18. When it is desired to remove the material from the container 18, the valve 17 is closed, and the valve 20 opened, and the material allowed to drop into any suitable car or other receptacle 25, the valve 22 being left open sufficiently to permit enough hydrogen gas to pass into the chamber 18, to replace the material removed therefrom. 'I he hydrogen gas produced by the reaction passes from the cooling pipes 23 and is then stored in the as tank 24, to be used as desired.

T e basic silicate obtained in the first step of the process is then mixed with a suitable slag-forming element, such as lime, magnesia or other material of calcareous nature,

and a suitable reducing agent, such as sili-.

con (ferro-silicon may be used), in about the following molecular proportions:

All of the materials are finely ground. This mixture is then fed into an electric furnace and the mass heated. -When a temperature of about 2000 F. is reached, the mass reacts and it is believed forms a calcium silicate, containing a small proportion of sodium silicate, but most of the sodium is liberated in the form of metal vapor, which distils out of the furnace and is then condensed in a suitable condenser. The temperature of the condenser may be so regulated as to hold the metallic sodium in the form of a liquid until a suitable quantity thereof is condensed, and

it may then be tap ed ofi into molds, or

otherwise convenient y removed. The conat apcylindrical brick work 28 is tamped a bedof coke 29, and above this a bed of lime 30, which forms the bottom of the furnace. Extending up throu h the bed of lime and normally protected y the superposed slag is one electrode 31 of the furnace, which at its bottom is electrically connected to an iron bar 32, which in turn is suitably connected to a source of'alternating electric current. Wrapped around the iron cylinder 26 are about eight layers of asbestos paper 33. It has been found that electrodes of a character adapted to conduct current economically and withstand the necessary temperature to apply electrical energy to the mass, sucl'bfor instance as graphite electrodes, are rapidly attacked by the cooling metal vapors at points removed from the hot ends of the electrodes if the metal vapors are allowed to come in contact therewith and particularly wherever the metal vapor is permitted to condense in or on the electrode. The other electrode is shown at 34, and in order that this may be protected from the action of the metallic vapor, it is surrounded by a thicklayer of powdered lime 35, and at its bottom portion by a thick layer 36 of powdered lime containing about 10% of finely powdered ferrosilicon, the lime and ferro-silicon being held in place by an iron shell. The carbon or graphite electrode 34 may be adjusted by means of a weight 37, connected to the electrode by means of a rope 38 passing over a pulley 39. The electrode is suitably connected to the source of electrical energy, by means of a flexible conductor 40. The cylindrical member 26 is preferably about thirty inches high and thirty inches in diameter.

The mixture of basic silicate, lime and reducing agent is fed into a hopper 41, leading to inlet pipe 42, into which extends a plunger or ram 43, which may be operated back and forth by hand, to gradually feed the material 44 from the pipe 42 into the electric furnace. One method of judging whether the temperature in the furnace is at the desired point, is to observe the color of the wrought iron shell 26. For this purpose holes 45 are cut through the asbestos paper 33, so that the wrought iron may be seen. When the mixture is heated in the electric furnace to about 2000 F., the vapor boiling of metallic sodium is produced, leaving calcium silicate as a slag and this slag may be tapped oil from time to time, throu h the slag opening 47 see Fig. 3), whic slag opening may be fil ed up with lime or powdered slag when it is not in use. The metallic vapors are conducted to a condenser 48, consisting of a six inch wrought iron pipe connected directly with the cylinder 26. and being inclined downwardly about one inch to the-foot, and being about twelve feet long. In order to-keep this pipe at the proper temperature, to maintain the condensed sodium in liquid form, a gas pipe 49 is provided therebeneath, with gas-jets impinging gas flames upon the pipe 48 to keep it at the desired temperature. Connected at the lower end of the pipe 48 is a T-head 50, having a two inch pipe 51 leading from the top" thereof. and a three-quarter inch pipe 52 leading from the bottom thereof, the top of the pipe 52 being adapted to be closed by a ball-valve 53 carried upon a stem 54, operated by a lever 55. Upon raising the ballvalve 53, the metallic sodium in liquid form will run into the cast iron molds 56 placed beneath the pipe 52 for collecting the same. Should the metallic sodium tend to freeze in the pipe 52, or above the ball-valve 53, a

gas jet 57, flexibly connected, may be di-- rected'against these parts in order to melt the metallic sodium and cause it to flow freely down to the. molds 56. In view of the fact that there may be some little caustic soda which has not been transformed into basic silicate in the first step, small amounts of hydrogen gas may be given oil from the electric furnace, which gas will escape through the pipe 51 and may be burned at the end thereof. The lower end of the pipe 48 should be kept at about 100 C. while the upper end may be red hot from the condensed sodium. The molds 56 may be wiped inside with a little oiland graphite, to permit of the easy removal of metallic sodium therefrom.

If it is desired to convert metallic sodium into peroxid, the apparatus shown in Figs. 4 and 5 may be used. Metallic sodium may be fed by hand into the pipesGO, at the right hand end, while hot air is passed through the pipes from the left hand end, causing the metallic sodium to burn to sodium peroxid. The air is first forced by means of a suitable fan or pump 61 over trays 62 in a suitable container, which trays contain lime or caustic soda in order to dry and purify the air. On leaving the trays 62, the air is forced through a pipe 63 into the right hand end of a chamber 64. surrounding the pipes 60. This chamber-is provided with suitable baflles 65 and 66, which bafiles have openings alternately at the top and bottom, so as to cause the air fromthe pipe 63 to pass back and forth transversely across the 68 at about 150 pipes 60, and thereby become heated. Upon reaching the left hand end of the apparatus, the warm air passes through apertures 67 and then through a perforated sheet 68 and into the left hand end of the pipes 60. The material is graduall fed through the 60 from right, to left, and shown in Fig. 4, by hand, by means of a two-tined rake and drops from the left hand end of the pipes 60 as peroxid, into a trough 69, from which it may be removed by a screw conveyer 70 into suitable cans or containers 71. The rate at which the air is introduced or forced through the apparatus by the fan is so regulated as to maintain the temperature of the air as it passes through the perforated plate C., while the temperature of the nitrogen and small quantities of oxygen leaving the pipe 60 at the right hand end should be about 250 C.

It will be seen from the above that the improved process in its preferred form contemplates taking any suitable compound of an alkali metal or the like, and heating it with any suitable reducin agent to a temperature sufficient to pro uce the vapor of the metal and .then condensing the vapor. By so choosing the compound and reducing agent that no gases are produced other than the metallic va or, very serious difliculties are avoided. a he gases would not only dilute the vapor, but it would be very diflieult to separate the gases from the metal vapor and other serious difliculties, as a manufacturing reposition, would result. Hence it is pref erred to treat. the starting material first with a de-hydrating agent to remove the hydrogen from the material. By this preliminary treatment it is possible to make metallic alkali metal from the by drates thereof, in a very simple and efficient manner. If'the starting material contains no h drogen or other gas forming elements, which would bedisadvantageous in the second step, it is only necessary to choose a suitable reducing agent which will not cause such gases to be roduced in the electric furnace, and for this urpose it is preferred to use a non-carboni erous reducing agent, such as silicon, as it then will not produce the oxids of carbon.

It will be understood that many chan es and modifications may be made without eparting from the spirit and scope of the invention in its broader aspects. Hence it is desired to cover all processes coming within the language of the appended claims.

at is claimed and desired to be socured by Letters Patent is:

1. The process of producing alkali metals which consists in heating a compound of an alkali metal with a reducing agent to produce alkali metal vapor, the alkali metal compound and silicious reducing agent being so chosen that substantially no gases, as

pipes.

distinguished from metal vapor are produced by the reaction, and then condensing the alkali metal vapor.

2. The process of producing alkali metals which consists in heating a basic silicate of the alkali metal with a reducing agent to produce alkali metal vapor, the reducing agent being so chosen that substantially no gases, as distinguished from metal vapor, are produced by the reaction, and then condensing the alkali metal vapor.

3. The process of producing alkali metals which consists in heatin a compound of an alkali metal with a silicon non-carboniferous reducing agent, the alkali metal compound being so chosen that substantially no gases, as distinguished from metal vapor, are produced by the reaction, and then condensing the alkali metal vapor.

4. The process of producing alkali metal which consists in heating a basic silicate thereof with a noncarboniferous reducin agent, to produce alkali metal vapor an then condensing the vapor.

5. The process of producing sodium which consists in heating a basic sodium silicate with a non-carboniferous reducing agent, and calcareous material, to produce metallic sodium vapor and then condensing the sodium vapor.

6. The process of producing metals from compounds thereof, which consists in heating in an electric furnace a basic silicate thereof with a suitable reducing agent sufiiciently to vaporize the metal therefrom, the compound and reducing agent being so chosen that substantially no gases, as distinguished from metal vapor, are produced by the reaction, and then condensing the metal vapor.

7. The process of producin alkali metals from compounds thereof, WhlCh consists in carrying out two steps in the first step, treating the alkali metal compound to alter it so that those elements are removed therefrom which would produce gases in the second step, and in the second step, heating the so prepared material with a reducing agent to vaporize the metal and condensing the metal.

8. The process of producin alkali metals from compounds thereof, WhlCh consists in dehydrating the compound, then heating the same in the 1presence of a reducing agent to produce al ali metal vapor and condensing the vapor.

. 9. The process of producing alkali metals from hydrated compounds thereof, which consists in dehydrating the compound, then heating it in the presence of a reducing agent to produce alkali metal vapor, the reducing agent being so chosen that substantially no gases, as distinguished from metal vapor, are produced by the reaction, and

then condensing the alkali metal vapor.

10. The process of producing alkali metals from hydrated compounds thereof, which consists in dehydratlng the compound, then heating it in the presence of a non-carboniferous reducing agent, to produce alkali metal vapor and condensin the vapor.

11. The process of producing alkali metals from hydrated compounds t ereof, which consists in dehydrating the compound, then heating it in the presence of a non-carboniferous reducing agent, and lime, to produce alkali metal vapor and condensin the vapor.

12. The process of (producing a ali metals from alkali metal hy rates which consists in treating the hydrate with silicon to produce a basic silicate of the alkali metal and then heating the basic silicate with a non-carboniferous reducing a cut, to produce alkali metal vapor and cominsing the vapor.

13. The process of producing alkali metals from alkali metal hydrates which consists in treating the hydrate with silicon to produce a basic silicate of the alkali metal and then heating the basic silicate with a reagent to produce alkali metal vapor and condensing the vapor.

14. The process of producing alkali metals from alkali metal hydrates which consists in treating the hydrate with silicon to produce a basic silicate of the alkali metal and then heating the basic silicate with a reducin agent to produce alkali metal vapor, the re ucln agent being so chosen that substantial y no gases, as distinguished from metal vapor, are produced b the reaction, and then condensing the alka i metal vapor.

15. The improved process which consists in heating a compound of an alkali metal with a reducing agent to produce alkali metal vapor, the alkali metal compound and reducing agent bein so chosen that substantially no gases, as istinguished from metal vapor, are produced by the reaction, and then condensing the alkali metal vapor and burning the metal to produce the peroxid thereo' 16. The improved process which consists in heating a basic silicate of an alkali metal with a non-carboniferous reducing agent, to produce alkali metal vapor, and burning the alkali metal to form peroxid thereof.

17. The process of producing alkali metals from compounds thereof, which consists in treating the compound with a reagent to produce a basic silicate thereof, and then heating the silicate with a non-carboniferous reducing agent to produce alkali metal,

metal vapor and condensing the metal vapor.

1,eee,eeo a 19. The recess of producing metal and pound thereof by means of electric current hydrogen m compounds thereof, which applied by electrodes adjacent the comconsists in tree the compound with a pound, to produce the metal in vapor form reagent to remove e hydrogen in the form and protecting the electrodes from the metal 5 of a substantially pure gas and then treatvapor in order to permit of the vapor being 15 ing the residue with a reduc' agent to condensed and recovered. vaporize the metal and then con ensmg the In testimony whereof, I have signed my metal. name to this specification.

20. The process of producing alkali metals .10 which consists in heating a. suitable com- WALTER L. MORRISON.

Cor'rectlons In Letters Patent No. 1,265,360.

It is hereby certified that in Letters Patent No. 1,255,360, granted May 7, 1918, upon the application of Walter L. Morrison, of Csnonsburg, Pennsylvania, for an improvement in "Processes for Producing Alkali Metals or the Like, errors appear in the printed spedficstion requiring correction as follows: Page 1, line 29, for the word "influential-y read jragmmtary; page, 3, line 12?, claim 1,

before the word "reducing insert the word eilicious; and that the said Letters latent should be read with these corrections therein that the some may conform to the record of the case in the Patent Olliee.

' Signed and sealed this 28th-dey of May, A. D., 1918.

, B. F. WHITEHF-AD,

Acting Uommiuioner of Petunia. 

